EP3455192B1 - Teil aus einem verbundwerkstoff mit keramischer matrix - Google Patents

Teil aus einem verbundwerkstoff mit keramischer matrix Download PDF

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Publication number
EP3455192B1
EP3455192B1 EP17727650.8A EP17727650A EP3455192B1 EP 3455192 B1 EP3455192 B1 EP 3455192B1 EP 17727650 A EP17727650 A EP 17727650A EP 3455192 B1 EP3455192 B1 EP 3455192B1
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EP
European Patent Office
Prior art keywords
silicate
matrix
phase
rare earth
mullite
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EP17727650.8A
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English (en)
French (fr)
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EP3455192A1 (de
Inventor
Eric Bouillon
Aurélia CLERAMBOURG
Lisa PIN
David Marsal
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Safran Ceramics SA
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Safran Ceramics SA
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    • C04B35/00—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products
    • C04B35/01—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics
    • C04B35/16—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay
    • C04B35/18—Shaped ceramic products characterised by their composition; Ceramics compositions; Processing powders of inorganic compounds preparatory to the manufacturing of ceramic products based on oxide ceramics based on silicates other than clay rich in aluminium oxide
    • C04B35/185—Mullite 3Al2O3-2SiO2
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Definitions

  • the invention relates to a part made of composite material that can be used at a high temperature, greater than or equal to 1300°C and for example between 1300°C and 1450°C.
  • the invention also relates to a method of manufacturing such a part as well as the use thereof.
  • CMC ceramic matrix composite materials
  • CVI Ceramic Vapor Infiltration
  • WO 2016/009148 discloses a process for manufacturing a part made of composite material by synthesis by self-sustaining reaction at high temperature
  • WO 2014/053751 discloses a method for manufacturing an aerodynamic part by overmolding a ceramic envelope on a composite preform
  • WO 2010/072978 discloses an environmental barrier for a silicon-containing refractory substrate
  • WO 2008/000247 discloses a method of protecting ceramic surfaces against corrosion.
  • the present invention aims to meet the aforementioned need.
  • the invention proposes, according to one of its aspects, a part made of composite material according to claim 1.
  • the invention advantageously makes it possible to provide a part compatible with use at a temperature greater than or equal to 1300° C. and which can be manufactured with a relatively limited production cost.
  • the matrix of the part comprising an environmental barrier material, the part according to the invention can be used in an oxidizing and humid atmosphere.
  • the matrix thus comprises at least one silicate phase.
  • This silicate phase is a mixed phase comprising a mixture of mullite (3Al 2 O 3 .2SiO 2 ) and at least one rare earth silicate.
  • said rare earth silicate may have the chemical formula: RE 2 SiO 5 or RE 2 Si 2 O 7 where RE denotes a rare earth element.
  • the rare earth silicate has the chemical formula RE 2 Si 2 O 7 .
  • the rare earth element RE can for example be chosen from: Y (yttrium), Er (erbium), Yb (ytterbium), Lu (lutetium) and Dy (dysprosium).
  • the rare earth element RE can be chosen from: Y, Yb and Lu.
  • the matrix implemented makes it possible to further reduce the production cost of the part, insofar as the incorporation of mullite into the matrix is more economical than the incorporation of a rare earth silicate.
  • the first phase can be located between the silicon carbide fibers and the second phase.
  • the first phase comprising mullite is located on the side of the fibers and the second phase comprising the rare earth silicate is located on the side of the outer surface of the part.
  • the matrix comprises a complementary phase of ceramic material matrix, different from the first and second sintered silicate phases, located between the silicon carbide fibers and the first and second sintered silicate phases.
  • the part can constitute a turbomachine part.
  • the part can be a part of the hot end of a gas turbine of an aeronautical engine or of an industrial turbine.
  • the part can constitute at least part of a distributor, a wall of a combustion chamber, a turbine ring sector or a turbine engine blade.
  • the present invention also relates to a method of manufacturing a part as described above according to claim 8.
  • At least part of the matrix is formed by sintering.
  • Such a characteristic advantageously makes it possible to manufacture the part by a technique with reduced implementation cost.
  • the entire matrix may be formed by sintering or, alternatively, only part of the matrix may be formed by sintering.
  • a temperature greater than or equal to 1200° C. can be imposed during sintering.
  • Such a characteristic is advantageous because it makes it possible to carry out significant sintering in order to further improve the mechanical properties of the part obtained.
  • Such a method makes it possible to manufacture a matrix comprising both mullite and a rare earth silicate and constitutes a solution making it possible to obtain a part having the desired properties with a particularly low implementation cost.
  • the present invention also relates to a method of using a part as described above, in which the part is used at a temperature greater than or equal to 1300°C, and for example between 1300°C and 1450°C.
  • the part can in particular be used in an oxidizing and humid atmosphere.
  • the part can advantageously be devoid of an environmental barrier coating during its use.
  • the matrix confers, in fact, the resistance to corrosion sought for the part.
  • it does not depart from the scope of the present invention if the part is used while being provided with an environmental barrier coating.
  • the silicon carbide fibers having an oxygen content less than or equal to 1% in atomic percentage can for example be fibers supplied under the name “Hi-Nicalon-S” by the Japanese company NGS. These fibers are hereinafter referred to as “SiC fibers”.
  • the fibrous reinforcement can be produced in a single piece by three-dimensional or multilayer weaving or from a plurality of two-dimensional fibrous strata or even from several layers of one-dimensional fabric.
  • the fibrous reinforcement can, for example, have a multi-satin weave, that is to say be a fabric obtained by three-dimensional weaving with several layers of weft yarns, the basic weave of each layer of which is equivalent to a weave of the classic satin type but with certain points of the weave which bind the layers of weft threads together.
  • the fibrous reinforcement may have an interlock weave.
  • weave or interlock fabric is meant a 3D weaving weave in which each layer of warp threads binds several layers of weft threads with all the threads of the same warp column having the same movement in the plane of the armor.
  • Different multi-layer weaving modes that can be used to form the fibrous reinforcement are described in particular in the document WO 2006/136755 .
  • fibrous textures such as two-dimensional fabrics of SiC fibers or unidirectional sheets of SiC fibers, and to obtain the fibrous reinforcement by draping such fibrous textures on a form.
  • These textures may optionally be bonded together, for example by stitching or implantation of threads to form the fibrous reinforcement.
  • the SiC fibers can be coated with an interphase present between the SiC fibers and the matrix.
  • the interphase can be monolayer or multilayer.
  • the interphase may include at least one layer of pyrolytic carbon (PyC), boron nitride (BN), boron nitride doped with silicon (BN(Si), with silicon in a mass proportion between 5% and 40%, the balance being boron nitride) or carbon doped with boron (BC, with boron in an atomic proportion between 5% and 20%, the balance being carbon).
  • the interphase here has a function of weakening the composite material which promotes the deflection of any cracks reaching the interphase after having propagated in the matrix, preventing or delaying the breaking of fibers by such cracks.
  • the matrix densifies the fibrous reinforcement by being present in the porosity of the latter.
  • the matrix comprises at least one continuous silicate phase coating the fibers of the fibrous reinforcement. SiC fibers are present in the matrix.
  • the matrix occupies the majority (i.e. more than 50%) of the accessible porosity volume of the fibrous reinforcement. In particular, the matrix can occupy more than 75%, or even substantially all, of the volume of this accessible porosity.
  • the matrix comprises at least one silicate phase comprising a mixture of mullite and at least one rare earth silicate.
  • the matrix may also advantageously comprise a complementary matrix phase of ceramic material located between the fibers (or the interphase) and the silicate phase.
  • This additional phase makes it possible to further improve the mechanical properties of the part made of composite material.
  • This complementary phase is formed of a material different from that constituting the silicate phase.
  • This complementary phase can comprise a carbide or a nitride.
  • This additional phase may, for example, comprise SiC, Si 3 N 4 , SiN(O), SiC(B) or a mixture of such compounds.
  • the matrix may be devoid of such a complementary phase.
  • the matrix consists of at least 50% by weight of a mixture of mullite and at least one rare earth silicate.
  • the matrix may consist of at least 80% by weight of a mixture of mullite and at least one rare earth silicate.
  • the matrix can, at inevitable impurities, being entirely constituted by a mixture of mullite and at least one rare earth silicate.
  • the matrix comprises a single rare earth silicate or several silicates of the same rare earth or of different rare earths.
  • the rare earth silicate(s) may or may be of the form: RE 2 SiO 5 or RE 2 Si 2 O 7 where RE denotes a rare earth element.
  • RE can for example be chosen from: yttrium Y, scandium Sc and lanthanides, such as for example ytterbium Yb, lutetium Lu, dysprosium Dy, erbium Er and lanthanum La.
  • the rare earth silicate(s) may advantageously be of the form RE 2 Si 2 O 7 with RE chosen from the list: Y, Yb and Lu.
  • a first step 10 may consist in producing the fibrous reinforcement formed by the SiC fibers.
  • the fibrous reinforcement of the part can be obtained from at least one textile operation using the SiC fibers.
  • the fibrous reinforcement can be obtained by multilayer or three-dimensional weaving of SiC fibers.
  • a step 20 of surface treatment of the SiC fibers, prior to the formation of the interphase, is preferably carried out in particular to eliminate the size present on the fibers.
  • Step 30 consists in forming an interphase of debrittlement by CVI on the SiC fibers forming the fibrous reinforcement.
  • This interphase can be in PyC.
  • the thickness of the interphase can for example be between 10 nm and 1000 nm, and for example between 10 nm and 100 nm.
  • the fibrous reinforcement remains porous, the initial accessible porosity being filled only for a minority part by the interphase.
  • a step 35 is then carried out in which the complementary ceramic matrix phase is formed in the pores of the fibrous reinforcement, on the interphase which has been formed beforehand.
  • This complementary phase can be formed by CVI.
  • an impregnating composition is introduced, for example in the form of a slip, into the pores of the fibrous reinforcement by methods known per se, for example by injection.
  • the impregnating composition may comprise a powder suspended in a liquid medium or be in the form of a solution.
  • the impregnation composition is intended to provide the constituents useful for forming the silicate phase of the matrix.
  • the impregnating composition may comprise a binder in a manner known per se.
  • the composition of the impregnation composition is determined according to the composition of the silicate phase to be obtained.
  • the impregnation composition may comprise at least one of the following constituents: powder of a rare earth silicate, sol-gel precursor of a rare earth silicate, mullite powder, sol-gel precursor of mullite, mixture of these compounds.
  • the impregnation composition may, in particular, comprise (a) a mixture of a mullite powder and a mullite sol-gel precursor, or (b) a mixture of a mullite powder and a precursor sol-gel rare earth silicate, or (c) a mixture of a powder of a rare earth silicate and a sol-gel precursor of a rare earth silicate, or (d) a mixture of a powder of a rare earth silicate and a sol-gel precursor of mullite, or (e) a mixture of a powder of mullite and a powder of a rare earth silicate, or alternatively (f) a mixture of a sol-gel precursor of a rare earth silicate and a sol-gel precursor of mullite.
  • the fibrous reinforcement Once the fibrous reinforcement has been impregnated, the latter is dried and debinded, then the silicate phase is formed by sintering (step 50).
  • a first heat treatment is carried out at a lower temperature making it possible to convert the sol-gel precursor(s) into mullite and/or rare earth silicate powder.
  • the temperature imposed during sintering is advantageously greater than or equal to 1200°C, for example between 1200°C and 1400°C.
  • the SiC fibers constituting the fibrous reinforcement have the degree of thermostability required not to be damaged during the sintering step at such temperatures.
  • the fact of sintering the powder present in the fibrous reinforcement above 1200° C. further improves the mechanical properties exhibited by the silicate phase formed.
  • the sintering can, for example, be carried out in air.
  • steps 10, 20, 30 and 35 are identical to those described in relation to the figure 1 .
  • a first impregnation composition is introduced into the pores of the fibrous reinforcement (step 140).
  • the first impregnation composition is as described above.
  • the first impregnation composition is intended to provide the useful constituents for forming a first silicate phase of the matrix after sintering (step 150).
  • a second impregnation composition different from the first impregnation composition, is introduced into the pores of the fibrous reinforcement (step 160).
  • the second impregnation composition is as described above.
  • the second impregnation composition is intended to provide the useful constituents for forming a second silicate phase of the matrix after sintering (step 170).
  • the second silicate phase is formed of a material different from that constituting the first silicate phase.
  • All of the first and second silicate phases can occupy more than 50%, for example more than 75%, for example substantially the entire volume of the accessible porosity of the fibrous reinforcement.
  • the first silicate phase can comprise mullite and the second silicate phase can comprise at least one rare earth silicate.
  • the first silicate phase may include at least one rare earth silicate and the second silicate phase may include mullite.
  • Mullite can represent between 10% and 25% of the volume of the composite material part.
  • the rare earth silicate can represent between 5% and 30% of the volume of the composite material part.
  • the silicate phase(s) it is possible to produce, after formation of the silicate phase(s), a matrix phase consolidating agent which makes it possible to further improve the cohesion of the matrix obtained.
  • a matrix phase consolidating agent which makes it possible to further improve the cohesion of the matrix obtained.
  • the heat treatment comprises firstly the transformation of the sol-gel precursor into the material of the consolidating matrix phase to be obtained and then the sintering of the material thus obtained in order to form the consolidating matrix phase.
  • the part can be a static or rotating part of a turbomachine.
  • turbomachine parts according to the invention have been mentioned above.
  • the part obtained can be used at a temperature greater than or equal to 1300°C, for example between 1300°C and 1450°C, for example between 1300°C and 1400°C.
  • a temperature greater than or equal to 1300°C, for example between 1300°C and 1450°C, for example between 1300°C and 1400°C.
  • the part is used at a temperature below 1300°C.
  • the fibrous reinforcement is first formed and then at least one impregnating composition is introduced into the pores of the latter.
  • the patent further describes cases where the part is shaped differently.
  • the SiC fibers could be impregnated with an impregnation composition as described above, then the fibrous reinforcement could be produced by filament winding of the SiC fibers thus impregnated.
  • the fibrous reinforcement could then undergo a step of drying and debinding then the sintering could be carried out as described above in order to obtain the part made of composite material.
  • unidirectional layers could be formed from SiC fibers impregnated with an impregnating composition as described above.
  • the fibrous reinforcement could then be obtained by draping the unidirectional layers thus formed, then the part could be formed by sintering as described above.
  • the fibrous reinforcement could be formed by draping a plurality of two-dimensional fibrous strata preimpregnated with the impregnating composition.
  • an interphase can of course be formed or not on the SiC fibers before impregnation with the impregnation composition, this interphase being as described above.

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Claims (12)

  1. Teil aus Verbundwerkstoff, das mindestens umfasst:
    - eine Faserverstärkung, die Fasern aus Siliziumkarbid umfasst, die einen Sauerstoffgehalt von unter oder gleich 1 % in Atomprozent aufweisen, und
    - eine Matrix, die in der Porosität der Faserverstärkung vorhanden ist und zu mindestens 50 Ma% aus einem Gemisch aus Mullit und mindestens einem Seltene-Erde-Silikat besteht, wobei die Matrix über 50 % des Volumens der zugänglichen Porosität der Faserverstärkung belegt, wobei die Matrix mindestens eine erste gesinterte Silikatphase umfasst, die Mullit umfasst, und eine zweite gesinterte Silikatphase, die sich von der ersten Phase unterscheidet, die mindestens ein Seltene-Erde-Silikat umfasst.
  2. Teil nach Anspruch 1, wobei das Seltene-Erde-Silicat als chemische Formel RE2SiO5 oder RE2Si2O7 hat, wobei RE ein Seltene-Erde-Element bezeichnet.
  3. Teil nach Anspruch 2, wobei RE aus Y, Yb und Lu ausgewählt ist.
  4. Teil nach einem der Ansprüche 1 bis 3, wobei sich die erste Phase zwischen den Siliziumkarbidfasern und der zweiten Phase befindet.
  5. Teil nach einem der Ansprüche 1 bis 4, wobei die Matrix umfasst:
    eine komplementäre Matrixphase aus Keramikwerkstoff, die sich von der ersten und zweiten gesinterten Silikatphase unterscheidet, die sich zwischen den Siliziumkarbidfasern und der ersten und zweiten gesinterten Silikatphase befindet.
  6. Teil nach einem der Ansprüche 1 bis 5, wobei das Teil ein Teil einer Turbomaschine bildet.
  7. Teil nach Anspruch 6, wobei das Teil ein Teil mindestens eines Verteilers, einer Wand einer Brennkammer, eines Turbinenringsektors oder einer Turbomaschinenschaufel bildet.
  8. Verfahren zur Herstellung eines Teils nach einem der Ansprüche 1 bis 7, das mindestens einen Schritt des Bildens der Matrix in der Porosität der Faserverstärkung umfasst, wobei die Matrix zu mindestens 50 Ma% aus einem Gemisch aus Mullit und mindestens einem Seltene-Erde-Silikat besteht und über 50 % des Volumens der zugänglichen Porosität der Faserverstärkung belegt, und wobei die Matrix mindestens durch die Durchführung der folgenden Schritte gebildet wird:
    - Einleiten mindestens eines Pulvers eines ersten Silikats oder mindestens eines Sol-Gel-Vorläufers eines ersten Silikats in die Porosität der Faserverstärkung,
    - Sintern des ersten eingeleiteten oder nach Umwandlung des Sol-Gel-Vorläufers erhaltenen Silikats, um eine erste Matrixphase zu bilden, die das erste Silikat umfasst,
    - Einleiten mindestens eines Pulvers eines zweiten Silikats oder mindestens eines Sol-Gel-Vorläufers eines zweiten Silikats in die Porosität der von der ersten Matrixphase verdichteten Faserverstärkung, und
    - Sintern des zweiten eingeleiteten oder nach Umwandlung des Sol-Gel-Vorläufers erhaltenen Silikats, um eine zweite Matrixphase zu bilden, die das zweite Silikat umfasst,
    und wobei das erste Silikat Mullit ist und das zweite Silikat ein Seltene-Erde-Silikat ist oder wobei das erste Silikat ein Seltene-Erde-Silikat ist und das zweite Silikat Mullit ist.
  9. Verfahren nach Anspruch 8, wobei eine Temperatur von über oder gleich 1200 °C während des Sinterns erforderlich ist.
  10. Verfahren nach einem der Ansprüche 8 oder 9, wobei das erste Silikat Mullit ist und das zweite Silikat ein Seltene-Erde-Silikat ist.
  11. Verwendung eines Teils nach einem der Ansprüche 1 bis 7, wobei das Teil bei einer Temperatur von über oder gleich 1300 °C verwendet wird.
  12. Verwendung nach Anspruch 11, wobei das Teil in einer oxidierenden und feuchten Atmosphäre verwendet wird.
EP17727650.8A 2016-05-11 2017-05-11 Teil aus einem verbundwerkstoff mit keramischer matrix Active EP3455192B1 (de)

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FR1654200A FR3051187B1 (fr) 2016-05-11 2016-05-11 Piece en materiau composite
PCT/FR2017/051128 WO2017194886A1 (fr) 2016-05-11 2017-05-11 Pièce en matériau composite a matrice céramique

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US11591270B2 (en) 2019-02-08 2023-02-28 Raytheon Technologies Corporation Doped silicon carbide ceramic matrix composite
WO2021075411A1 (ja) * 2019-10-17 2021-04-22 株式会社Ihi セラミックス基複合材料及びその製造方法
CN113526972A (zh) * 2021-07-28 2021-10-22 中国科学院上海硅酸盐研究所 一种抗强烧蚀的稀土改性超高温陶瓷基复合材料及其制备方法

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JPH02296770A (ja) * 1989-05-12 1990-12-07 Ngk Spark Plug Co Ltd 高温耐酸化性セラミックス複合材料
JPH05269716A (ja) * 1992-03-27 1993-10-19 Sumitomo Metal Ind Ltd セラミックス複合材料の製造方法
US7063894B2 (en) * 2003-05-22 2006-06-20 United Technologies Corporation Environmental barrier coating for silicon based substrates
US20050129973A1 (en) * 2003-12-16 2005-06-16 Eaton Harry E. Velocity barrier layer for environmental barrier coatings
FR2887601B1 (fr) 2005-06-24 2007-10-05 Snecma Moteurs Sa Piece mecanique et procede de fabrication d'une telle piece
DE102006030235B4 (de) * 2006-06-30 2008-04-10 Fraunhofer-Gesellschaft zur Förderung der angewandten Forschung e.V. Verfahren zum Schutz von Heißgaskorrosion von keramischen Oberflächen oder eines Körpers, hochtemperaturbeständiger Körper und deren Verwendung
FR2940278B1 (fr) * 2008-12-24 2011-05-06 Snecma Propulsion Solide Barriere environnementale pour substrat refractaire contenant du silicium
FR2996549B1 (fr) * 2012-10-04 2016-01-29 Herakles Procede de fabrication d'une piece aerodynamique par surmoulage d'une enveloppe ceramique sur une preforme composite
EP2970017B1 (de) * 2013-03-15 2019-07-10 Rolls-Royce Corporation Sic-basierte keramikmatrix-verbundstoffe mit geschichteten matrizen und verfahren zur herstellung sic-basierter keramikmatrix-verbundstoffe mit geschichteten matrizen
CN103755344B (zh) * 2013-10-12 2017-01-11 北京航空航天大学 单硅酸镥/焦硅酸镥双相复合环境障涂层材料及其制备方法
FR3023961A1 (fr) * 2014-07-17 2016-01-22 Herakles Procede de fabrication d'une piece en materiau composite par synthese par reaction auto-entretenue a haute temperature
CN104446670B (zh) * 2014-11-28 2016-10-05 中国人民解放军国防科学技术大学 C/SiC复合材料表面涂层体系及其制备方法
CN104529498B (zh) * 2014-12-17 2016-08-31 南京航空航天大学 放电等离子烧结一步制备多层环境障碍涂层的方法
FR3041890B1 (fr) * 2015-10-05 2017-11-24 Snecma Procede de fabrication d'une piece en materiau composite par injection d'une barbotine chargee dans un moule poreux

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FR3051187B1 (fr) 2018-06-01
CN109476552B (zh) 2022-12-13
JP6987785B2 (ja) 2022-01-05
US10988417B2 (en) 2021-04-27
US20190152861A1 (en) 2019-05-23
EP3455192A1 (de) 2019-03-20
JP2019522608A (ja) 2019-08-15
FR3051187A1 (fr) 2017-11-17
CN109476552A (zh) 2019-03-15
WO2017194886A1 (fr) 2017-11-16

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